1253907-79-7Relevant articles and documents
Preparation method of landiolol hydrochloride intermediate
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Paragraph 0026, (2021/06/06)
The invention discloses a preparation method of a high-purity landiolol hydrochloride intermediate N-(2-aminoethyl)-4-morpholinecarboxamide oxalate. The preparation method comprises the following steps: reacting N-phenoxy carbonyl morpholine with ethylenediamine, concentrating the reaction liquid, adding a solvent for dissolving, adjusting the pH value to 9-14 by using alkali, filtering to remove solid byproducts, concentrating the filtrate to obtain N-(2-aminoethyl)-4-morpholine formamide, adding water for dissolving, adjusting the pH value to 1-6 by using oxalic acid, filtering to remove a small amount of ethylenediamine oxalate solid, concentrating the filtrate, adding a solvent, and recrystallizing to obtain the high-purity N-(2-aminoethyl)-4-morpholinecarboxamide oxalate. According to the method, the high-purity landiolol hydrochloride intermediate can be obtained, the defects that the byproduct sodium phenate is difficult to filter, ethylenediamine is easy to remain and the like are overcome, the process is stable and controllable, the solvent can be recycled, and the method is more suitable for industrial production.
Preparation method of landiolol hydrochloride
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Paragraph 0074-0083, (2021/03/03)
The invention discloses a preparation method of landiolol hydrochloride, which comprises the following steps of by using a nitrogen-containing organic compound hydrochloride as a hydrogen chloride carrier, salifying to obtain landiolol hydrochloride. According to the preparation method disclosed by the invention, complex operations such as insufficiency during two-phase salifying and organic phasedrying are avoided, the risk of disqualification of physicochemical items is reduced, the production period is shortened while solid wastes are reduced, the operation is easier, and the cost is lower; dangerous operation and concentration operation of hydrogen chloride organic solution preparation are avoided, the preparation condition is mild, and the risk that related substances exceed the standard is reduced; the chromatographic purity of the product can reach 99.7% or above, and the yield is 80% or above, so that the method is more suitable for industrial production.
Method for preparing landiolol hydrochloride
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, (2019/12/02)
The invention belongs to the field of pharmaceutical chemicals, and particularly relates to an improved method for preparing landiolol and a compound shown as a formula 8. The compound shown as the formula 8 is prepared by reacting a compound shown as a formula 7 with AH (organic amine). The invention also relates to compounds of general formula 7.
Preparation method of landiolol hydrochloride
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Paragraph 0066-0068; 0073, (2018/11/22)
The invention relates to a preparation method of landiolol hydrochloride, in particular to the selection of a reaction solvent 1,4-dioxane. The landiolol hydrochloride prepared by means of the methodcan prevent the generation of ester exchange impurities, the operation is simple, the reaction yield is high, the method is suitable for industrial large-scale production, and a crude drug and the preparation of the crude drug have better safety performance, effectiveness and stability, and have significant use in preparing drugs used for urgently treating arrhythmia and postoperative dynamic monitoring abnormality.
Process for the enantioselective synthesis of landiolol
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, (2018/06/28)
PROBLEM TO BE SOLVED: To provide a process for the enantioselective synthesis of landiolol.SOLUTION: The process for the enantioselective synthesis of landiolol represented by formula (B) uses a compound represented by formula (A) as an intermediate.
Preparation method of landiolol hydrochloride
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, (2017/08/14)
The invention provides a preparation method of landiolol hydrochloride. The preparation method utilizes cheap and easily available raw materials. A key reaction utilizes a phase transfer catalysis method so reaction time is shortened. The preparation meth
Process for the enantioselective synthesis of landiolol
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Paragraph 0053; 0054; 0055; 0056; 0057, (2014/02/15)
A process for the preparation of Landiolol 1, ((S)-2,2-dimethyl-1,3-dioxolan-4-yl)methyl 3-(4-((S)-2-hydroxy-3-(2-(morpholine-4-carboxamido) ethylamino)propoxy)phenyl)propanoate) starting from (S)-(2,2-dimethyl-1,3-dioxolan-4-yl)methyl 3-(4-hydroxyphenyl)propanoate, an alkylating agent with epoxide structure, in particular epichlorohydrin, and 2-(morpholine-4-carboxamido)ethanamine in the form of the free base or of a salt thereof. Said process is carried out without isolating most intermediates, does not require chromatographic purifications and is particularly advantageous in terms of yields and productivity. Furthermore, the resulting Landiolol is particularly pure and can be conveniently transformed into Landiolol hydrochloride with high enantiomeric purity.
